先进表征技术在锆合金显微组织研究中的应用进展

Application Progress of Advanced Characterization Techniques in Microstructural Studies on Zirconium Alloys

摘要:

锆合金具有良好的核性能、力学性能和加工性能，是一种重要的结构材料，在核工业、航空航天和医疗设备等领域中应用前景广泛。深入了解锆合金显微组织对于掌握其性能和性质至关重要，其显微组织（如第二相、氧化膜、氢化物等）在加工和服役过程中的演变规律及对性能影响正得到材料科学、核工程领域研究者的广泛关注。先进表征技术，如电子显微分析技术、电子探针显微技术、原位表征技术及原子探针分析技术等已被应用于锆合金显微组织研究。电子显微分析技术，可对锆合金包壳的第二相、氢化物和氧化膜的显微组织特征进行表征，为锆合金包壳材料性能的优化改进提供支持。电子探针显微技术（EPMA）是高分辨率显微技术，可对锆合金的微观结构及表面特征进行分析。原位表征技术，包括透射电子显微镜原位辐照技术、原位电化学阻抗谱技术、原位拉伸实验和原位拉曼光谱。透射电子显微镜原位辐照技术，可用于研究锆合金在辐照条件下的行为及辐照引起的微观结构变化；原位电化学阻抗谱技术，可用于研究锆合金在腐蚀过程中的阻抗模量及氧化膜厚度的变化；原位拉伸实验，可实时观察锆合金的变形行为；原位拉曼光谱，可用于检测锆合金成分及结构的变化。原子探针分析技术，可对锆合金中元素偏聚现象、氧化过程、氢的分布及纳米尺度下原子分布情况的表征。综述了先进表征技术在锆合金微观组织研究中的应用进展及存在的问题，展望了锆合金显微组织的未来研究方向。本研究为深入了解锆合金的微观结构提供了参考，深化了对锆合金组织结构及性能的认识。

Abstract:

Zirconium alloy has good nuclear，mechanical，and machining properties. As an important structural material，it has a wide application prospect in the nuclear industry，aerospace，and medical equipment. Understanding the microstructure of zirconium alloy is crucial to understanding their performance and properties. The microstructural changes（such as second phase，oxide film，hydride，etc.）under processing and service conditions and the effects on properties have attracted extensive attention in the fields of materials science and nuclear engineering. Advanced characterization methods play a key role in the study of the microstructure of zirconium alloys. In recent years，advanced characterization methods including electron microscopy，electron probe microanalysis，in-situ characterization，and atom probe have developed rapidly，and have been applied in the study of zirconium alloy microstructures，providing people with a deeper understanding of the structure and properties of zirconium alloys. Electron microscopic analysis technology can characterize the microstructural characteristics of the second phase， hydrides，and oxide films of zirconium alloy cladding，providing support for the optimization and improvement of the performance of zirconium alloy cladding materials. Electron probe microanalysis（EPMA） is a high-resolution microscopic technique that can analyze the microstructure and surface characteristics of zirconium alloys. In-situ detection techniques include in-situ irradiation technology with transmission electron microscopy， in-situ electrochemical impedance spectroscopy technology，in-situ tensile experiments，and in-situ Raman spectroscopy. Among them，in-situ irradiation technology with transmission electron microscopy can be used to study the behavior of zirconium alloys in irradiation conditions and the microstructural changes caused by irradiation. In-situ electrochemical impedance spectroscopy technology can be used to study the changes in impedance modulus and oxide film thickness of zirconium alloys during corrosion. In-situ tensile experiments can observe the deformation behavior of zirconium alloys in real time，and in-situ Raman spectroscopy can be used to detect changes in the composition and structure of zirconium alloys. Atom probe tomography can analyze the element segregation phenomenon，oxidation process，hydrogen distribution，etc. in zirconium alloys，as well as characterize the atomic distribution at the nanoscale. In this paper，the application progress and existing problem of characterization methods in the study of zirconium alloy microstructure are reviewed. The future research direction of zirconium alloy microstructure is prospected based on engineering practice， providing a reference for an in-depth understanding of the microstructure of zirconium alloy.